WO1979000801A1 - Corps ligneux mineralises et methode de fixation d'un depot mineral sur des surfaces de fragments de bois - Google Patents

Corps ligneux mineralises et methode de fixation d'un depot mineral sur des surfaces de fragments de bois Download PDF

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Publication number
WO1979000801A1
WO1979000801A1 PCT/EP1979/000018 EP7900018W WO7900801A1 WO 1979000801 A1 WO1979000801 A1 WO 1979000801A1 EP 7900018 W EP7900018 W EP 7900018W WO 7900801 A1 WO7900801 A1 WO 7900801A1
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Prior art keywords
fragments
mineral
cement
ammonium
product
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PCT/EP1979/000018
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German (de)
English (en)
Inventor
L Paszner
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Thermoform Bau Forschungsgesel
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Application filed by Thermoform Bau Forschungsgesel filed Critical Thermoform Bau Forschungsgesel
Priority to BR7907479A priority Critical patent/BR7907479A/pt
Publication of WO1979000801A1 publication Critical patent/WO1979000801A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/32—Phosphorus-containing compounds

Definitions

  • Woody plant structures comprise arrays of hollow cells (tracheids) having fiber constituents comprised as cellu lose which is present as high-polymer strong micro-fibril wall structure surrounded by non-fiber carbohydrate, constituents which encompass the lignins, sugars, starches, extractives, proteins, polyphenolics, resins, waxes, fatty substances, and gums.
  • Various sequestered minerals may also be occluded, chiefly silica.
  • the fragments may be crtimb-like saw generated particles and riusts; rough lumps, slivers and dusts made by hammer milling or hogging; pulp fibers.made by wet grinding; and shavings, veneers, strands, wood-wools and excelsiors made by slicing with knife-edge tools.
  • Typical treatments hitherto resorted to comprise: Ca) impregnating fragment surfaces with soluble motal salts suc as Chlorides of calcium or magnesium, which hasten the se of hydraulic cement slurry adjacent the frajuirnntj (b) digesting extractables at and near fragment surfaces by trujuirnntj with baths of lime or caustic soda, with or without further stabilizing by a pozzolan or a polyvnl ⁇ nt metal salt; and (c) loading surfaces of fragments with a mineral gel, eg sodium silicate.
  • a mineral gel eg sodium silicate
  • the prior art has proposed dry cement compositions comprising phosphorous containing c ⁇ mpounds including phosphoric acid, and basic metal oxides such as aluminum and magnesium oxides and their oxyphosphate compounds, settable on rnixing with water to form a concrete binder, as disclosod in United States patent 3,525,632 dated August 25, 1970 issued to Enoch, CR Such cements are intended to b ⁇ ur.ed with mineral aggregates.
  • a number of prior workers have combined water-soluble or dissolved acid phosphates with magnesia in rapid-setting compositions incorporating refractory fillers.
  • a fast-setting concrete of low porosity disclosed in United States patent 3,879,209 issued April 22, 1975 to Limes et al, is made with 15 parts by weight of 34 percent P 2 0 5 ammonium polyphosphate solution and an equal weight of 150 mesh magnesia, admixed with 70 parts limestone, dolomite, sand, or gravel, 3 parts salt, and 15 parts water; such concrete develops an early set and high compressive strength in a few hours.
  • the binding together of mineral solids by a cementing agent essentially requires that such agent be a viscous liquid, paste, or slurry, capable of wetting all surfaces of the mineral solids while plastic, and capable of gelation and development of interlocked crystal groups adhered to at least some portions of the aggregate materials Cast bodies have high compressive strengths due to the effective support column created by the cement matrix surrounding the aggregate grains, but low tensile strength due to relatively low shear strengths of the bonds.
  • the product inherently includes voids. If very great compaction pressures are applied, the void volume may be less than 10%; however when assemblies having densities of 0.5 to 0.9 are desired the ratio of internal spaces to total molded volume may ranks from 30 to 75% or more. It will be evident that the stress-resisting structure is weakened by the presence of such voids as compared to a specimen of whole, clear wood.
  • the ability of the composite molded assembly to resist an applied load will depend on the ability of the fragments as laid up and on the junction bond cross-section and strength to withstand the localized stresses.
  • the directions of principal tensile and compressive stresses do not follow smooth curves, as in an ideal homogeneous beam, because of the presence of voids. Consequently, in light-weight molded structural products the bond adhesion to fragment surfaces, and the actual strength of the binder itself, are the critical parameters which determine the capacity of the molded product to resist loads.
  • the span length is a large multiple of the beam depth in panels and boards, and since the constituent fragments will usually have thickness dimensions a small fraction of the beam depth, a large number of linked fragments are involved in a three-dimensional chain or lattice resisting the tensile stress, the fragments and their associated bond bridges located along the lower mid-span surface carrying the largest bond l ⁇ ads.
  • a similar chain or lattice adjacent the upper beam surface at mid-span opposes the largest compressive stresses.
  • a facing sheet of veneer or paper is adhered such member obviously shields the outer chains from part of the stress.
  • any stress-resisting chain will be less than the fragment cross-sectional areas.
  • the bond bridges will have different directions, ie the fragment contact planes will usually not be parallel with the direction of the principal tensile stress, hence the bridges will be subjected to varying proportions of shear ing and tensile stresses. Because a chain is no stronger than its weakest link it may be seen that those bond bridges subjected solely or mainly to tension represent concentrated stress regions limiting the flexural strengt of the product.
  • each fragment will be irregular and will comprise partly crushed, deformed, and fissured fiber groups, presenting a relatively large area of openings extending into the woody fragment as compared to the minimum enclosing surface for the fragment volume.
  • Such individual fragments therefore represent lignocellulosic fiber structure which is signif icantly less strong than the volumes of wood in the plant or tree before the fragment was removed. It becomes highly desirable, therefore, that the setting of the binder mass around and upon the fragment should enhance the flexural and compressive strengths as well as the flexural and compressive moduli of elasticity.
  • the nature of the desired junction bond should be such as to lock the domain of binder between and surrounding fragments integrally to the greatest possible surface area of the fragments; this implies a substantial penetration by binder material into all fissures, apertures and pores opening to fragment surfaces, and no degradation of the strength of binder material by extractables present in the plant materials.
  • the present invention contemplates a process for making an adhered mineral cladding layer on a surface area of a ligneus body by applying to the surface an amount of ammonium polyphosphate aqueous solution -sufficient to initially wet the surface and a dep ⁇ sit of particulate mineral solids such as magnesium or caicium oxide, or magnesium or caicium hydroxide or magnesium or caicium carbonate in an amount to form a clinging layer adhered to the wet surface, and drying the body.
  • particulate mineral solids such as magnesium or caicium oxide, or magnesium or caicium hydroxide or magnesium or caicium carbonate
  • the invention in a principal aspect envisages the use of ligneus material which has a moisture content in the ranks between essentially dehydrated state and about 100% by weight of water, and also envisages use of particulate mineral solids in an amount of between about 15 mg and 200 mg of Mg0 per cm 2 of the ligneus surface of grain sizes ranging between 149 microns and about 15 microns, with an amount of solution supplying from 12 to 20 mg of P 2 0 5 per cm 2 of surface.
  • the invention may be understood to provide a ligneus body having in its pore spaces a deposit of ammonium phosphate salt and having a surface volume of metal oxyphosphate compounds of a metal which may be magnesium or caicium crystallized in micro-cavit ies and recesses in the surface volume, the body having an adhere mineral deposit of particulate solids bonded together and to the body by said compounds.
  • a still further aspect of the invention shows that the invention as recited may provide the body with a salt deposit of 40 mg to 70 mg per cubic centimeter of wood volume and an adhered mineral deposit ranging from about 65 to 400 mg per square centimeter of body surface area.
  • the role of the binder is mainly to resist shearing stresses , which increase generally toward the span ends.
  • the adhesion of the binder should be such that a significant shear failure of wood should result when the product is tested to rupture rather than shear failure of the bond.
  • the present invention is directed to improved bond formation between a wide ranks of lignocellulosic materials available in nature and mineral binder masses cementihg fragments of such materials together as porous compositions.
  • the invention is directed especially to providing concreted lignocellulose fragment assemblies which have exceptionally high strength properties, as represented by the Modulus of Rupture in bending, while at the same time having light weight and low cost.
  • the invention is also directed to novel methods of admixing a basic metal compound such as magnesium or caicium oxides, hydroxides and carbonates with a phosphate compound so as to anchor a metal ⁇ xyphosphate-cemented bond mass intimately to lignocellulose fragment surfaces, resulting in high bond shear strength.
  • a basic metal compound such as magnesium or caicium oxides, hydroxides and carbonates
  • a phosphate compound so as to anchor a metal ⁇ xyphosphate-cemented bond mass intimately to lignocellulose fragment surfaces, resulting in high bond shear strength.
  • the invention is to be understood as providing for the application of the mineral solids as an initial layer of magnesium or caicium oxide, hydroxide or carbonate followed by a second deposit of larger grain sizes and weight per unit area, the initial solids being of particle sizes ranging from sub-micronic to a few microns and in amount of from about 1.5 mg to about 3.5 mg per cm 2 of body surface.
  • the invention can be further comprehended as providing a process for attaching a metal oxyphosphate mineral binder mass as an integral cladding on the surfaces of ligneus fragments bonding to the fragment surfaces a mineral solids layer, and for imparting strength enhancement, fire retardancy and decay-resistant properties to the fragments by an impregnation treatment of fragment surfaces with an aqueous solution of ammonium polyphosphate and a deposition of the mineral solids layer comprised of a magnesium or caicium compound reactive with the solution to form metal oxyphosphate binder compounds, the solids being of grain sizes in a range from sub-micronic to about 250 microns.
  • the invention also, contemplates processes for attainment of low density structural composites of board form having a core portion of wood fragments incorporating surface impregnating amounts of an electrolyte supplying phosphate ions and carrying an adherent binder mass formed by the reaction of caicium or magnesium oxide, hydroxide or carbonate grains applied as a surface deposit with the electrolyte, the binder mass bridging fragment portions as junction bonding masses, the core portion being bonded to veneer sheets of wood by the binder mass.
  • sheet-li .ke lignocellulose fragments are utilized having contacting surfaces impregnated with an adhered integral mineral binder mass comprised of the reaction products with ammonium polyphosphate solution and caiciumor magnesium oxides, hydroxides or carbonates.
  • a liquid ammonium polyphosphate consisting of 65 to 85% of P 2 0 5 combined as polyphosphates, and 25 to 30% as orthophosphates, or by different amrnoniation a salt product having P 2 0 5 content about equally divided between ortho- and polyphosphate salts may be made.
  • These products are highly reactive with the basic alkaline earth metal oxides, hydroxides and carbonates, especially those of magnesium and caicium, and the reaction products formed as thin coatings, classified as metal oxyphosphates, are water resistant and strong and are deemed superior to those of Portland cement.
  • microcrystalline salt deposit extending into wood spaces to a depth of from a few hundred microns to several millimeters as partial or total filling of pits, limina, and formed coatings on vessel walls.
  • Such deposit attributes not only significant in- creases in compressive and bending strengths of the woody material, but confers much needed fire-retarding properties to the wood.
  • Substantial transport of colloid matter is effected by liquid issuing from the porous reservoirs characterizing ligneous matter contiguous to the cement grains, and by reabsorption of liquid into the wood.
  • This mechanism enables the distribution of reaction products and loading of pore spaces of a woody substance thereby, in a manner quite dissimilar to the formation of a binding mass around refractory aggregate particles from a surrounding solution of ammonium polyphosphate.
  • the solution is carried as a partial filling of hollow tracheid spaces in wood and the surface of the wood carries grains of Mg0 and mineral extender grains, an outward migration of liquid occurs which causes lively local motion of wetting films which move about grain surfaces and carry suspended colloid masses.
  • the migration appears to be effected both by capillary transport of the suspending liquid or by mechanically induced pressure gradients therein, and by electrostatic forces within the electrolyte Solutions. A signif icantly large transport of such masses deposites them at some distance from the grains within the wood pores.
  • a critical temperature must be reached befqre gelation takes place.
  • the time interval between the wet paste stage and its actual solidification may vary considerably, as the gel transition tends to depend on factors such as the composition of the grain mixture, the ratios and amounts of grain sizes, the concentrati ⁇ n of the dissolved ammonia, and the temperature of the mixture. In all cases large surface, small grain sizes hasten the gelation whereas inert components moderate the reaction rate to a considerable extent. Thus setting rates can be effectively varied by judicious selection of the reaction conditions and the composition of the reactants.
  • Continuous casting processes may use a grain mixture (hereinafter referred to as "cement solids") with high proportion of Mg0 of high density relative to the inert or weakly inert grain portion.
  • the Mg0 preferably would be of highly reactive state, as represented by USP grade material or dead-burned dense grain rather than merely calcined rnagnesite.
  • inert or weakly reactive filler solids there may be used magnesite of raw form, or a dolomite, or other inert solids of suitable particle sizes such as silica, zirconia, alumina, and alkaline earth metal phosphates and silicates and mixtures thereof in the ratio of a fraction of the amount of Mg0 up to 100 times the weight of Mg0.
  • Ammonium carbonate which has been shown to be formed by combination of magnesium carbonate with ammonium polyphosphates, is a weak electrolyte which migrates freely in liquid occupying wood spaces, eventually lodging as a crystalline deposit of the salt within tracheids and wood pore which deposit augments the residual fire retardant effect of ammonium polyphosphate compounds in the wood after curing, if an excess solution has been supplied.
  • Variations in the early strength are reflecting the intrinsic particle strengths rather than interferance of some wood constituents with the bonding process as noted in the prior art with Portland cement and other magnesite cements.
  • Samples of the same wood spe cies having different product densities were made with 1, 2 and 10 kg / cm 2 compaction pressures at the time of casting.
  • Tests No. 1 and 2 show that high quality low density products are realizable with relatively low reactant costs.
  • a series of boards was made using oriented ligneous fragments derived from sugarcane rind, this being the exterridl fibrous stalk portion lying radially inwardly of a hard waxy and silicaceous skin layer, having thi ⁇ kness ranging from about 1.3 to 2.8 mm.
  • the inside pith and. ⁇ utside waxy layers were removed by mechanical action and the Strands having cross sectional area of 1.5 to. 5 mm and thickness of 1.0 to 2.0 mm and length was chopped to 15-20 cm mechanically.
  • Fire-retardant low density structural board products were made from sugarcane residue, i.e., bagasse resulting from mechanical expression of cane juices by passing the stalks which have been stripped of leaves -through crushing rollers, and water rinsing. The pressed stalks were subsequently hammermilled into random particles comprising the rind fiber structure, pith and all other components of the plant found with the rind, ie. waxes and silicaceous deposites normally present.
  • the hammermilled fragments had particles ranging to 8 cm in length with thickness between 1 to 4 mm. Dust and fine fragments smaller than 20 mesh in size were removed by screening. The specific gravity of the bagasse was estimated at 0.21 and the surface area was determined at 19,000 cm 2 per 100 g of air-dry fragments.
  • a test quantity of 200 g of the air-dry fragments was treated with 360 g of commercial fertilizer grade ammonium polyphosphate solution of specific gravity 1.4 and analysis of 10:34:00 NPK, supplying about 9.5 mg of solution per square centimeter of enveloping surface , equivalent to a film thickness of 68 microns, supplying 3.23 mg P 2 0 5 per cm 2 fragment surface.
  • a cement solids mixture of 150 g of djead burned magnesia and 450 g of powdered dolomite passing 100 mesh was s-ifted onto the polyphosphate wetted fragments and tumble mixed for 22 sec.
  • the quantity of Mg0 grain as judged from its measured density of 3.36 was inferred to furnish 11.5% or 17.3 g reactable Mg0 as oxyphosphate; accordingly 132.7 g serving only as dense inert support filier.
  • the dolomite was inferred to contribute 10.5 g Mg0 to the reaction, the remainder being inert filier (428 g).
  • the bagasse cement mixture was immediately dumped into a flanged board mold measuring 15 cm by 30 cm, leveled, and compacted by a pressure plate with 7.5 kg / cm 2. Thickness waiis held at 2.53 cm. The pressure was released after 12 mi: in and the board was air-dried for five days before testing. The temperature of the board at the time of stripping- from the mold was 54 ° C. The resulting board product had a cured volume of 1017 cm 3 and weighed 998 g, indicating a bulk density of 0.98. The MOR and MOE values obtained in static bending were 79.4 and 17,900 kg / cm 2 , respectively.
  • a computation of the residual ammonium polyphosphate (neglecting the ammonium carbonate formed from dolomite) solution remaining as dried salt crystallized within the pores of the bagasse indicates that an amount in excess of that needed to meet Class A fire rating for lignocellulosics was held in the fragments . Accordingly, the product was tested for flammability by exposing it to direct flame of 800 ° C temperature over an area qf 4.5 cm by 4.5 cm for 15 min. At the e ⁇ d of that time only minor surface scorching was evident without flaming. Minor gas evolution and steaming was evident initially as the flameside became red hot while the opposite side was only slightly warm at 40 ° C.
  • Ammonium polyphosphate in solid form such as TVA 's 11:55:00 or 12:54:00 is also useful as impregnating salt and in onestep admixing of caicium and magnesium compounds with fragments, salt and water to affect their bonding.
  • the MOR and MOE values were 18.6 and 10,200 kg / cm 2 , respectively.
  • the second set of samples was alternately immersed in tap and sea water with air-drying between the soakings. A total of 7 such cycles were performed and the resulting samples finally tested in bending in air-dry condition. The reduction in MOR was 7% and the weight loss recorded was 3% for the weathered portion.
  • the relatively high bonding rates possible with the present invention make continuous casting of mineral bonded wood products of high strength and light weight having hollow circular or rectangular shapes such as used for drainage tiles, culverts and longer pipe sections possible. Useful ness of this inyen.tion for such applications becomes especially evident as porosity and permeability to fluids is made technically possible by selecting manufacturing conditions under which such light weight tubes can be fabri- cated. On the other hand, by selecting conditions under which migration of colloids to product surfaces is promoted, as in processes of spin casting, closed surfaces tiles and tubes can be made.
  • the continuous molding process may include low RPM spinning of the mold during or after the casting to cause simultaneous densification of the wood cement mixture and set up colloid migration to the surface on account of the centrifugal force created thereby.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Dry Formation Of Fiberboard And The Like (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
  • Fireproofing Substances (AREA)

Abstract

Le procede de fabrication de produits de structure coules vegetaux/mineraux ayant des proprietes de retardement de l'inflammation utilise une majeure partie en volume de fragments de vegetaux ligneux, tels que des bois tendres et durs, de la canne a sucre, des tiges de plantes cereales et fibreuses, et une partie mineure en volume d'un depot d'un liant mineral comprenant des oxyphosphates de magnesium ou de calcium et des particules de materiau de remplissage inerte. Des fragments ayant des epaisseurs allant de 0,3 mm a 8 mm et consistant en eclats, copeaux, languettes, brins, faisceaux de fibres, fibres, feuilles de placage epluchees et sciees subissent une application sur leurs surfaces d'une solution aqueuse de polyphosphate d'ammoniaque ou d'un sel phosphate acide soluble fournissant de 0,15 a 0,40 parties de P2O5 comme ion phosphate par partie de fragments en poids, et des particules solides de ciment consistant en MgO ou CaO ou Mg(OH)2 ou Ca(OH)2 ou MgCO3 ou CaCO3 en quantites variant de 0,25 a 1 partie par partie de fragment, et de 0,01 a 0,80 partie de particules de remplissage inertes; le melange est place dans un moule et maintenu sous une pression de compactage predeterminee jusqu'a ce que le produit devienne rigide, en 10 minutes environ. Un plus grand retardement de l'inflammation est obtenu lorsque la solution de phosphate est principalement absorbee dans les surfaces des fragments avant que les particules solides de ciment soient saupoudrees sur les surfaces mouillees. Avec des pressions de compactage faibles le produit en vrac a une faible densite et une structure ouverte. L'utilisation de MgO de densite 2,8 ou plus, d'une dimension de maille de -100 a +250 et de polyphosphates d'ammoniaque d'analyse 10:34:00 ou 11:37:00 avec des fragments seches a l'air ou au four en quantite suffisante pour garder des quantites de sels impregnes de sechage jusqu'a 65 milligrammes par centimetre cube de materiau ligneux, permet d'obtenir un produit solide et a grand retardement d'inflammation. Les produits moules par les procedes selon l'invention peuvent avoir toutes les formes de structure courantes telles que les planches, panneaux, plaques, poutres et blocs ainsi que les cadres, armatures, montants, tubes et pratiquement toutes les configurations pouvant etre coulees. De tels produits peuvent etre economiques a fabriquer, ne necessitant que peu ou pas de melange dans une vaste gamme de densites de produits, en fonction du degre de compactage maintenu pendant le tassement et ne necessitant que peu de temps pour le moulage et le durcissement. De tels produits, apres durcissement sont resistants aux flammes, ne se decomposent pas, sont resistants aux intemperies et ne sont pas attaques par les termites.
PCT/EP1979/000018 1978-03-20 1979-03-20 Corps ligneux mineralises et methode de fixation d'un depot mineral sur des surfaces de fragments de bois WO1979000801A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
BR7907479A BR7907479A (pt) 1978-03-20 1979-03-20 Processo para a fabricacao de um artigo composto moldado

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CA299288 1978-03-20
CA299,288A CA1081718A (fr) 1978-03-20 1978-03-20 Structures ligneuses ayant un revetement mineral, et methode de fixer un depot mineral aux surfaces de bois fragmentees

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Publication Number Publication Date
WO1979000801A1 true WO1979000801A1 (fr) 1979-10-18

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PCT/EP1979/000018 WO1979000801A1 (fr) 1978-03-20 1979-03-20 Corps ligneux mineralises et methode de fixation d'un depot mineral sur des surfaces de fragments de bois

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US (1) US4339405A (fr)
EP (1) EP0004372B1 (fr)
JP (1) JPS6251908B2 (fr)
AR (1) AR218114A1 (fr)
AT (1) AT372066B (fr)
AU (1) AU534506B2 (fr)
CA (1) CA1081718A (fr)
CS (1) CS222671B2 (fr)
DD (1) DD142537A5 (fr)
DE (1) DE2966654D1 (fr)
ES (1) ES478766A1 (fr)
FI (1) FI62525C (fr)
HU (1) HU182555B (fr)
IN (1) IN151462B (fr)
NZ (1) NZ189941A (fr)
PH (1) PH17288A (fr)
PL (1) PL125974B1 (fr)
RO (1) RO79468A (fr)
WO (1) WO1979000801A1 (fr)
YU (1) YU64379A (fr)

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PH17288A (en) 1984-07-06
US4339405A (en) 1982-07-13
AU534506B2 (en) 1984-02-02
ATA202979A (de) 1983-01-15
DD142537A5 (de) 1980-07-02
EP0004372B1 (fr) 1984-02-15
AR218114A1 (es) 1980-05-15
FI62525C (fi) 1983-01-10
EP0004372A1 (fr) 1979-10-03
PL214254A1 (fr) 1980-01-02
CA1081718A (fr) 1980-07-15
AU4525479A (en) 1979-09-27
AT372066B (de) 1983-08-25
RO79468A (fr) 1982-07-06
IN151462B (fr) 1983-04-23
NZ189941A (en) 1982-12-07
HU182555B (en) 1984-02-28
DE2966654D1 (en) 1984-03-22
FI790893A (fi) 1979-09-21
PL125974B1 (en) 1983-06-30
YU64379A (en) 1983-01-21
JPS6251908B2 (fr) 1987-11-02
ES478766A1 (es) 1979-11-01
JPS55500171A (fr) 1980-03-27
FI62525B (fi) 1982-09-30
CS222671B2 (en) 1983-07-29

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